Trabajo presentado en: 10th World Congress of Chemical Engineering, 1 a 5 de octubre de 2017, Barcelon

Paz Barragán, Esther de

Spanish

Repositorio Institucional de la Universidad de Burgos

10th World Congress of Chemical EngineeringBarcelona 2017STUDY OF THE OXIDATION OF AN OMEGA-3 CONCENTRATE AFTER FORMULATION AS OIL IN WATER EMULSIONSEsther de Paz University of Burgos, SpainIncorporation of fishoil to food productsStrategiesIntroductionOmega-3 polyunsaturatedfatty acids(n-3 PUFA)Fish oil,Natural sourceEPA (C20:5n-3) and DHA (C22:6n-3)Essential fatty acidsn-3 PUFA entirelyderived from dietFood habits: meat, fastfood, snack food…Rich in saturated fatty acidsLow proportion PUFAImportance in human healthReduction risk of cardiovascular diseases and cancer, improve brain development, preventioninflammatory related pathologiesNutritionists: necessity of consuming fish and greenvegetables to prevent manydiseasesDevelopment of productsenriched with n-3 PUFANutritional suplementsFuctional foodsIntroductionHighly susceptible to lipidoxidation, in presence of oxygen and temperature Negative impact on shelf life, nutritional value and flavor of foodsLow water solubilityDisadvantages(n-3 PUFA)RequiredFormulationn-3 PUFAAvoid or delay oxidationImprove dispersability in water systemsObjectivesDevelopment of an optimum formulation of anomega-3 concentrate as oil in water emulsion Study of the oxidative stability of the emulsion over time Study of the effect of antioxidants addition to thedeveloped formulation on the oxidative stability over timeCarrier material: OSA-starchOmega-3 concentrateCommercial Omega-3 polyunsaturated fatty acids (n-3 PUFA) concentrateTotal content of DHA: 73%Total n-3 PUFA: 92%72 % triglycerides11% diglicerides2% monoglycerides15% ethyl estersPeroxide value3.79 ± 0.017 meq O2/kg oilAnisidine value11.94 ± 0.065Oxidation stateSuitable forhuman consumptionExperimental SectionPreparationOSA-starchdissolutionAddition of oilphase (ω-3 concentrate)Pre-mixingPre-emulsionEmulsificationbyUltrasoundsStudy the effect of amplitude, ultrasounds time and oil content on the droplet sizeOptimalemulsionExperimental DesignResponse Surface Methodology(RSM)Optimal conditions by RSMOil content (X1): 3-9 % w/w (total solids: 30% w/w)Ultrasounds emulsification time (X2) : 60-300 sAmplitude (X3): 50-100%Effect of different variables on droplet size (Y) Optimal conditionsR2= 96,1715%Oil content: 6 % w/wUltrasounds time: 180 sAmplitude: 100%Predicted Value: 116 nmExperimental value: 121 nmCentral Composite Design17 experimental settings3 replicates in central pointSecond order polynomial equation: prediction response values of dropletsize as a fuction of X1, X2 and X3. Analysis of variance with 95% confidence levelDroplet size ↓ when amplitude ↑ (at X2= 180s)Droplet size ↓ when ultrasounds time ↑Optimal conditions by RSMEffect of different variables on droplet size (Y) Analysis of variance with 95% confidence levelY = a0 + a1X1 + a2X2 + a3X3 + a11X12 +a22X22 + a33X32 + a12X1X2 + a13X1X3 + a23X2X3Central Composite Design17 experimental settings3 replicates in central pointOil content (X1)3-9 % w/w (total solids: 30%)Ultrasounds emulsificationtime (X2)60-300 sAmplitude(X3)50-100%Second order polynomial equation: prediction response values of dropletsize as a function of X1, X2 and X3. Effect of variables on droplet sizeDroplet size ↓ when amplitude ↑ Droplet size ↓ when ultrasounds time ↑Droplet size ↓ when oil content ↓All coefficients statistically significantException: a11, a33 and a13Optimal conditions by RSM10203010011012013014015016017050 60 70 80 90 100Droplet size (nm)Amplitude (%)160-170150-160140-150130-140120-130110-120100-110 60 120 180 240 3001001201401601802001015202530Droplet size (nm)180-200160-180140-160120-140100-120Droplet size ↓ when amplitude ↑ (at X2= 180s)Droplet size ↓ when ultrasounds time ↑Time: 180 s Amplitude: 75%Optimal conditionsR2= 96,1715%Oil content: 6 % w/wUltrasounds time: 180 sAmplitude: 100%Predicted Value: 116 nmExperimental Value: 121 nmOptimal emulsion stability during storage024681012140,01 1 100Volume(%)Emulsion Droplet size distribution (µm)0 days2 days6 days29 daysSmall poblation of higher droplet size≈ 120 nmCreaming: from 6 daysafter emulsion preparationOxidative stability of emulsion Opening the oil container and handling without N2 atmosphere Emulsion storage at ambient temperature and darkness0102030405060700 2 4 6 8 10Peroxides value (meq O2/kg oil)Storage time (days)00,511,522,533,544,50 2 4 6 8 10TBARS Value(mmol/kg oil)Storage time (days) At t = 0 days, PV ↑↑  High values of PV and TBARS over timePreliminary studyRequired to open and handle the oilcontainer with N2Oxidative stability of emulsion Open and handle the oil container with N2 atmosphere Emulsion storage at ambient temperature and darkness0,00,51,01,52,00 1 2 3 4 5 6 7 8PV value(meqO2/kgoil)Storage time (days)0,01,02,03,04,00 2 4 6 8 10 12TBARS value(mmol/kg oil)Storage time (days) Constant PV over time (PV= 1-1.5 meq O2/kg oil) TBARS values increase considerably from 7th day of storage PV at t=0 days > PV oil (3.8 meq O2/kg oil) Formulation protectsagainst oxidation of omega-3 concentrateOxidative stability of emulsionEmulsion with addition of Ascorbic Acid (20 mM)0,01,02,03,04,00 2 4 6 8 10 12Peroxides value (meq O2/kg oil)Storage time (days)0,00,51,01,52,02,53,00 2 4 6 8 10 12TBARS Value(mmol/kg oil)Storage time (says) Storage with N2 and T=4ºC Storage at ambient temperature and darkness Slighly lower PV and TBARS values when emulsion was stored with N2 and at 4ºC. Almost constant values of PV with addition of AA as reported in literature (Uluataet al. 2015).  TBARS values were constant over time, similar to ω-3 concentrate TBARS value(0.825 ± 0.033 mmol/kg)SuitableFormulationConstant values and similar to ω-3 concentrate The formulation of ω-3 concentrate as oil in water emulsionsadding AA, was suitable to delay the lipid oxidationOxidative stability of emulsionComparative: Emulsion with addition of Ascorbic Acid (20 mM), ɑ-tocopherol(1.75 mg/g oil) and control emulsion0,00,51,01,52,02,50 1 2 3 4 5 6 7 8 9PV value(meqO2/kgoil)Storage time (days)0,01,02,03,04,00 2 4 6 8 10 12TBARS value(mmol/kg oil)Storage time (days)Control emulsion Emulsion with Ascorbic Acid Emulsion with ɑ-tocopherol Similar values of PV comparing with the control emulsion. The addition ofantioxidants to the emulsion did not affect to the primary oxidation Control and ɑ-TOC emulsions similar TBARS values. Adding ɑ-TOC to emulsions did not delay the secondary oxidation Adding AA to emulsions delays the secondary oxidationEmulsion storageTamb and darkness Development of a suitable formulation of an omega-3 concentrate as oil in water emulsions by ultrasounds Optimum emulsion (120 nm): 6% oil content, 180s of ultrasoundsemulsification time and 100% amplitude Oxidative stability of emulsion Preliminary study Under N2 atmosphere, PV decreased comparing with the preliminary study(PV= 1-1.5 meq O2/kg oil)  Effect of adding different antioxidants Addition of Ascorbic Acid: contant values of PV and TBARS (and similar to the ω-3 concentrate) Addition of ɑ-tocopherol: similar values of PV and TBARS comparedwith control emulsionConclusionsFormulation protects againstoxidation of ω-3 concentrateSuitable to delay thelipid oxidationRequired to open and handle the oilcontainer under N2 atmosphereTHANK YOU FOR YOUR ATTENTIONAcknowledgments: • To JCyL and EDRF for financial support of Project BU055U16 and OB´s contract• To Spanish government for EDP´s (FJCI-2014-19850) and RM´s (BES-2013-063937) contracts• To UBU for AGS´s contract10th World Congress of Chemical EngineeringBarcelona 2017STUDY OF THE OXIDATION OF AN OMEGA-3 CONCENTRATE AFTER FORMULATION AS OIL IN WATER EMULSIONSEsther de Paz University of Burgos, Spain

Study of the oxidation of an omega-3 concentrate after formulation as oil in water emulsions

https://riubu.ubu.es/bitstream/10259/4904/1/Paz-study_of_oxidation.pdf

Study of the oxidation of an omega-3 concentrate after formulation as oil in water emulsions

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